CN106256340A - A kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil and preparation method thereof - Google Patents

A kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil and preparation method thereof Download PDF

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CN106256340A
CN106256340A CN201610515437.8A CN201610515437A CN106256340A CN 106256340 A CN106256340 A CN 106256340A CN 201610515437 A CN201610515437 A CN 201610515437A CN 106256340 A CN106256340 A CN 106256340A
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oil
var
prunus armeniaca
ansu maxim
cortex eucommiae
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乌云塔娜
朱绪春
杜红岩
李铁柱
朱高浦
赵罕
杜兰英
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PAULOWNIA RESEARCH AND DEVELOPMENT CENTRE STATE FOREST BUREAU
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PAULOWNIA RESEARCH AND DEVELOPMENT CENTRE STATE FOREST BUREAU
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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  • Life Sciences & Earth Sciences (AREA)
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  • Dermatology (AREA)
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  • Gerontology & Geriatric Medicine (AREA)
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Abstract

Open a kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil of the present invention and preparation method thereof, including following component: Prunus armeniaca L.var.ansu Maxim. oil, Eucommia Oil, vitamin E acetate, caprylic/capric triglyceride, ethylhexyl palmitate, olive oil, essence and phenyl phenol & ethylhexyl glycerol.The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps: that vacuum emulsification pot is dried by (1), and the temperature of regulation vacuum emulsification pot is 80~85 DEG C, and pressure is 5~20 handkerchiefs;(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.Almond oil and eucommia ulmoides seed oil are effectively combined by the present invention, substantially increase the ageing resistace of skin, make skin keep elasticity, effectively reduce the anaphylactic reaction of skin simultaneously.

Description

A kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil and preparation method thereof
Technical field
The present invention relates to daily use chemicals product field.More particularly, to a kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil and preparation method thereof.
Background technology
True Beauty stems from the health of health, and a kind of life state that health is people to be unable to do without.Chinese traditional massage The physical therapy mode massaged, makes the health that people keep fit in enjoyment.Massage, is the important composition portion in theory of Chinese medical science Point, it is recovering physiotherapy, prevents health illness, away from a kind of maneuver of sub-health state.By different maneuvers and mode, to flesh Meat presses, and corrects skeleton, stimulates the specific meridians of human body, acupuncture point and echo area, regulation health, thus reaches to dispel The purposes such as wind is active, alleviation is uncomfortable, health invigorating.Moreover, massage may also operate as releiving pressure, loosen mood and Looks improving and the skin nourishing, toxin expelling etc. act on.
But during massage, can't do without certain medium, this medium is massage oil, it is protected in medical treatment The aspects such as strong massage are widely used.Massage oil is usually and uses plant or mineral oil, according to the one of purpose allotment Plant working fluid or semi-solid paste matter.It has skin care, improves skin lubrication degree, it is achieved body surface is massaged, and reduces Friction and obstruction, play a role in health care to skin simultaneously.Massage oil the most on the market is uneven, containing chemical industry synthetic Matter, although can play lubrication, but skin causes stimulation and injury, and assimilation effect is poor, makes people produce greasy tired Vexed sense, and expensive.
Summary of the invention
It is an object of the present invention to provide one and prevent skin aging, improve the Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil of skin elasticity And preparation method thereof.
For reaching above-mentioned purpose, the present invention uses following technical proposals:
A kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, is made up of following component: emollient and preservative.
Above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, described emollient includes Prunus armeniaca L.var.ansu Maxim. oil and the mixture of Eucommia Oil, vitamin E acetate, pungent Acid/tricaprin (GTCC), ethylhexyl palmitate, olive oil and essence.
Above-mentioned GTCC is commercially available prod, buys in Yu Xuan bio tech ltd, Guangzhou.
Above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, described preservative is phenyl phenol & ethylhexyl glycerol (PE9010).
Above-mentioned PE9010 is commercially available prod, buys in Guangdong Zhong Peng Chemical Co., Ltd..
Above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, is made up of the component of following mass fraction: Prunus armeniaca L.var.ansu Maxim. oil and the mixture 1.5 of Eucommia Oil ~3.0%, vitamin E acetate 0.3~0.7%, GTCC20~40%, ethylhexyl palmitate 30~50%, olive oil 20~ 35%, essence 0.014~the 0.21 of 0.035% and PE9010~0.38%.
Above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, the volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 6~0.2:1.
Above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, including the component of following mass fraction: Prunus armeniaca L.var.ansu Maxim. oil and the mixture of Eucommia Oil 2.0%, vitamin E acetate 0.5%, GTCC30%, ethylhexyl palmitate 40%, olive oil 27.2%, essence 0.02% and PE9010 0.28%, in the mixture of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil, Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil volume ratio are 3:1.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 80~85 DEG C, and pressure is 5~20 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
The preparation method of above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, described emollient includes Prunus armeniaca L.var.ansu Maxim. oil and the mixture of Eucommia Oil, VE Acetate, GTCC, ethylhexyl palmitate, olive oil and essence;Described preservative is PE9010.
The preparation method of above-mentioned Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, Prunus armeniaca L.var.ansu Maxim. oil and the mixture 1.5 of Eucommia Oil~3.0%, VE acetic acid Ester 0.3~0.7%, GTCC20~40%, ethylhexyl palmitate 30~50%, olive oil 20~35%, essence 0.014~ 0.035% and PE9010 0.21~0.38%;The volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 6~0.2:1.
The preparation method of eucommia ulmoides seed oil of the present invention is as follows:
(1) supercritical CO is used2Extraction process acquisition seed of bark of eucommia crude oil:
(1-1) seed of bark of eucommia supercritical CO2The pre-treatment of extraction: seed of bark of eucommia is dried and pulverized 40 mesh sieves and obtains seed of bark of eucommia Powder, first seed of bark of eucommia powder is immersed in temperature be 50-60 DEG C, polyvinyl alcohol mass fraction be 2-4wt% poly-vinyl alcohol solution in 0.5-1 hour, seed of bark of eucommia powder soak while carry out supersound process, ultrasonic frequency is 35KMz, ultrasonic power be 260~ 400W, filters and is dried to obtain seed of bark of eucommia powder, and polyvinyl alcohol is polyvinyl alcohol 1788 or polyvinyl alcohol 1799;Poly-vinyl alcohol solution Preparation method is as follows: be soaked in by polyvinyl alcohol in the ethanol solution that ethanol mass fraction is 70-85wt% 12-24 hour, mistake Filter is dried, and is then joined by the polyvinyl alcohol obtained in the water of 50-60 DEG C, and heated and stirred i.e. obtains poly-vinyl alcohol solution in 1 hour
(1-2) seed of bark of eucommia powder supercritical CO2Extraction: the seed of bark of eucommia powder obtained in step (1-1) is put in extraction kettle, Extraction process uses ethanol or ethanol volumetric concentration be 30~80% aqueous solution be entrainer, entrainer flow velocity is 1-3mL/ min;When being entrainer when using ethanol water, first the aqueous solution that ethanol volumetric concentration is 30% is passed through in extraction kettle, The most successively the aqueous solution that ethanol volumetric concentration is 40%, 50%, 60%, 70% and 80% is joined in extraction kettle, ethanol Aqueous solution that aqueous solution that volumetric concentration is 30%, ethanol volumetric concentration are 40%, ethanol volumetric concentration be 50% aqueous solution, Ethanol volumetric concentration be 60% aqueous solution, ethanol volumetric concentration be 70% aqueous solution and ethanol volumetric concentration be the water of 80% The ratio of the time that six kinds of ethanol waters of solution are passed through extraction kettle is: 2:3:1:1:1:2;Extracting pressure is 25~35MPa, extraction Temperature is 45~50 DEG C, and extraction time is 1.5~2.5h, and separating pressure is 6~7MPa, and separation temperature is 45~50 DEG C, obtains Seed of bark of eucommia crude oil;
(2) refine of seed of bark of eucommia crude oil, specifically comprises the following steps that
(2-1) being placed in heating tank by seed of bark of eucommia crude oil, be warming up to 60~70 DEG C, adding weight is seed of bark of eucommia crude oil weight 0.05-0.25wt ‰, concentration are the phosphoric acid of 80-90wt%, react 45~55min;
(2-2) the seed of bark of eucommia crude oil in heating tank is proceeded in outer tank, add the alkali liquor prepared in advance immediately, pour into Alkali liquor at the uniform velocity stirs on one side, and mixing speed is 40~50 turns/min, reacts 10~15min, settles 4~6h;
In this step: alkali liquor is NaOH solution, NaOH solution is 3:1~5:1/mL:g with the ratio of seed of bark of eucommia crude oil;Alkali Changing temperature is 70~80 DEG C;
In this step: total alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are Kg/h for oil flow, unit, and AV is seed of bark of eucommia crude oil Acid number, unit be mgNaOH/g;
B. phosphoric acid alkali consumption NP: owing to the addition of phosphoric acid in the degumming of this technique, therefore alkali liquor interpolation is considered as neutralising phosphoric acid consumption Alkali number;NP=1.22 × W, W are H3PO4Addition, unit are Kg/h, and the amount of phosphoric acid is pure phosphoric acid amount here;
C. excess alkali quantity NC: excess alkali is the 0.25~0.5wt% of oil mass, NC=Q × 25%, and Q for oil flow, unit is Kg/h;
Actual caustic soda amount NS: due to the Caustic soda purity on market, therefore should be according to its NaOH actual content when calculating Convert: the NaOH percentage composition of actual caustic soda amount NS=(N+NP+NC)/commercially available alkali;
(2-3) taking supernatant, adding NaCl mass fraction is the NaCl solution of 0.5-1.5wt%, NaCl solution addition For seed of bark of eucommia crude oil weight 5-15wt%, at the uniform velocity stir, rotating speed 40~50 turns/min, settle 2h;
(2-4) taking supernatant, be 0.06~0.095Mpa in vacuum, temperature is dried under conditions of being 90~110 DEG C;
(2-5) entering bleacher, in bleacher, vacuum is 0.06~0.095Mpa, and temperature is 90~110 DEG C, toward decolouring Tank adds seed of bark of eucommia crude oil and weighs the food grade active hargil of 2~4wt%, react 45~55min;
(2-6) open circulated filter system, be circulated filtration, clarifying to seed of bark of eucommia crude oil;
(2-7) entering in deodorizing tower, in deodorizing tower, vacuum is 0.0002MPa, temperature be 100~240 DEG C of reactions 3~ 5h;
In this step: deodorizing tower is to use physical refining tower, fatty acid supplementary set device to be applied in combination and carry out physical deacidification deodorize;
(2-8) being naturally cooling to 100~170 DEG C, water flowing is accelerated to be cooled to room temperature;
(2-9) it is polished filtering by bag filter, bestows the pressure of 4kg, filter, obtain seed of bark of eucommia refined oil;
In this step: in bag filter the material of filter bag film be polyphenylene sulfide fibre, polyimides, aramid fiber or One in polytetrafluoroethylene fibre;
In this step: in bag filter, the aperture size of filter bag film is 0.2~0.9nm.
The preparation method of mountain almond oil of the present invention is as follows:
(1) the de-bitter pre-treatment of Semen pruni armeniacae:
(1-1) Semen pruni armeniacae hulling machine shelling, first machine screening, then artificial screening obtains the Semen pruni armeniacae that shells;
(1-2) Semen pruni armeniacae is poured in 90~100 DEG C of hot water 60~120s, proceed to 4~10 DEG C of cold water impinging cooling 2~ 5min;
(1-3) being poured into by Semen pruni armeniacae in stripping machine and peel, first machine screening, then artificial screening obtains Prunus armeniaca L.var.ansu Maxim. of peeling Core;
(1-4) decortication Semen pruni armeniacae is poured in 90~100 DEG C of hot water carry out four times soak, in immersion process, water temperature is the coldest But;Soak 2~4h for the first time, rinse with tap water after pulling out;Second time soaks 10~12h, rinses with tap water after pulling out;The Soak 2~4h, rinse with tap water after pulling out for three times;Soak 2~4h, rinse with tap water after pulling out for 4th time;
(1-5) Semen pruni armeniacae of de-hardship is poured in drying pool, at 60~70 DEG C, air blast or microwave drying;During microwave drying, The frequency using microwave drying is 2000~2400MHz, power 1500~2800W, and the thickness of the bed of material is 6~7cm;
(2) mountain almond oil extraction refine:
(2-1) pretreatment after Semen pruni armeniacae takes off hardship: Semen pruni armeniacae was pulverized 50 mesh sieves and obtains Semen pruni armeniacae powder, soaks Semen pruni armeniacae powder Steep temperature be 50-60 DEG C, polyvinyl alcohol mass fraction be 2-4wt%, Polyethylene Glycol mass fraction be the poly-second of 5-10wt% In enol-polyglycol solution 0.5-1 hour, Semen pruni armeniacae powder carried out supersound process while soaking, and ultrasonic frequency is 35KHz, ultrasonic power is 260~400W, filters and is dried to obtain Semen pruni armeniacae powder, and polyvinyl alcohol is polyvinyl alcohol 1788 or poly-second Enol 1799, Polyethylene Glycol is polyethylene glycol 200, PEG400 or Macrogol 600;
The preparation method of polyvinyl alcohol-polyethylene glycol solution is as follows: it is 70-that polyvinyl alcohol is soaked in ethanol mass fraction In the ethanol solution of 85wt% 12-24 hour, filtering drying, then the polyvinyl alcohol obtained is joined in the water of 50-60 DEG C, Heated and stirred obtains poly-vinyl alcohol solution in 1 hour, obtains polyvinyl alcohol-polyethylene glycol molten after then adding Polyethylene Glycol stirring and dissolving Liquid;
(2-2) low temperature squeezes mountain almond oil: expressing process uses pure physical squeezing, and temperature controls between 35~55 DEG C, Solid-liquid is carried out the isolated Semen pruni armeniacae dregs of rice and supernatant;The Semen pruni armeniacae dregs of rice are joined in the water of its quality 3-6 times, utilize microwave Reactor controls the temperature 55 of material~60 DEG C, and being added thereto to account for Semen pruni armeniacae dregs of rice mass fraction is 0.055~0.065wt% Compound enzyme, enzymolysis 60~80min, it is centrifuged to obtain thick Semen pruni armeniacae crude oil, the frequency of microwave reactor is 2500~3000MHz, power 1600~2500W;Compound enzyme includes that the mass ratio of protease and cellulase, protease and cellulase is 1:3~2:5;Egg The mass ratio that white enzyme includes neutral protease and alkaline protease, neutral protease and alkaline protease is 1:1~2:3;
(2-3) mountain almond oil refine:
(2-3-1) supernatant and thick Semen pruni armeniacae crude oil are mixed, obtain Semen pruni armeniacae crude oil;
(2-3-2) Semen pruni armeniacae crude oil is warming up to 60~70 DEG C, adds Semen pruni armeniacae crude oil weight 0.05-0.15wt%, concentration For the phosphoric acid of 75-95wt%, react 25~35min;
(2-3-3) take the supernatant obtained in step (2-3-2), add the water of Semen pruni armeniacae crude oil weight 5-15wt%, at the uniform velocity Stirring, rotating speed is 40~50 turns/min, settles 2h;
(2-3-4) take the supernatant obtained in step (2-3-3), vacuum be 0.06~0.095Mpa, temperature be 90 ~be dried under conditions of 110 DEG C;
(2-3-5) enter bleacher, in bleacher vacuum be 0.06~0.095Mpa, temperature be 90~110 DEG C, add The food grade active hargil of Semen pruni armeniacae crude oil weight 2wt%~4wt%, reacts 25~35min;
(2-3-6) open circulated filter system, be circulated filtration, clarifying to filter liquor;
(2-3-7) enter in deodorizing tower, in deodorizing tower vacuum be 0.0002MPa, temperature be 100~240 DEG C, react 2 ~4h;
(2-3-8) being naturally cooling to 100~170 DEG C, water flowing is accelerated to be cooled to room temperature;
(2-3-9) it is polished filtering by bag filter, gives the pressure of 4kg, filter, obtain Semen pruni armeniacae Refined oil.
Beneficial effects of the present invention is as follows:
(1) rich in V in almond oilA、VE、VD3、VPIt is effective antioxidant and life Deng multivitamin, vitamin A and E Thing free radical scavenger, can effectively prevent skin aging, keep skin elasticity, make skin maintain vigour;
(2) rich in unsaturated fatty acid in eucommia ulmoides seed oil, wherein the content of alpha linolenic acid is up to more than 60%, is that human body must Needing fatty acid, it can promote skin growth, prevents skin aging, keeps skin elasticity, reduces skin allergy.
(3) almond oil and eucommia ulmoides seed oil are effectively combined by the present invention, substantially increase the ageing resistace of skin, make skin Keep elasticity, effectively reduce the anaphylactic reaction of skin simultaneously.
Detailed description of the invention
In order to be illustrated more clearly that the present invention, below in conjunction with preferred embodiment, the present invention is described further.Ability Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and should not limit this with this The protection domain of invention.
Part I: the preparation of eucommia ulmoides seed oil
A kind of eucommia ulmoides seed oil extracts refinery practice, comprises the steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil.
(1-1) seed of bark of eucommia supercritical CO2The pre-treatment of extraction: seed of bark of eucommia is dried and pulverized 40 mesh sieves and obtains seed of bark of eucommia Powder, first seed of bark of eucommia powder is immersed in temperature be 55 DEG C, polyvinyl alcohol mass fraction be 3wt% poly-vinyl alcohol solution in 1 hour, Seed of bark of eucommia powder carries out supersound process while soaking, and ultrasonic frequency is 35KMz, and ultrasonic power is 350W, filters and is dried Seed of bark of eucommia powder, polyvinyl alcohol is polyvinyl alcohol 1788 or polyvinyl alcohol 1799;The preparation method of poly-vinyl alcohol solution is as follows: will be poly- Vinyl alcohol is soaked in the ethanol solution that ethanol mass fraction is 80wt% 12 hours, filtering drying, the poly-second that then will obtain Enol joins in the water of 55 DEG C, and heated and stirred i.e. obtains poly-vinyl alcohol solution in 1 hour;
(1-2) seed of bark of eucommia powder supercritical CO2Extraction: the seed of bark of eucommia powder obtained in step (1-1) is put in extraction kettle, Extraction process uses ethanol or ethanol volumetric concentration be 30~80% aqueous solution be entrainer, entrainer flow velocity is 1-3mL/ min;When being entrainer when using ethanol water, first the aqueous solution that ethanol volumetric concentration is 30% is passed through in extraction kettle, The most successively the aqueous solution that ethanol volumetric concentration is 40%, 50%, 60%, 70% and 80% is joined in extraction kettle, ethanol Aqueous solution that aqueous solution that volumetric concentration is 30%, ethanol volumetric concentration are 40%, ethanol volumetric concentration be 50% aqueous solution, Ethanol volumetric concentration be 60% aqueous solution, ethanol volumetric concentration be 70% aqueous solution and ethanol volumetric concentration be the water of 80% The ratio of the time that six kinds of ethanol waters of solution are passed through extraction kettle is: 2:3:1:1:1:2;I.e.: always extraction time is the situation of 2h Under, aqueous solution, ethanol volumetric concentration that aqueous solution that ethanol volumetric concentration is 30%, ethanol volumetric concentration are 40% are 50% Aqueous solution, ethanol volumetric concentration be 60% aqueous solution, ethanol volumetric concentration be 70% aqueous solution and ethanol volumetric concentration be Six kinds of ethanol waters of the aqueous solution of 80% each lead into the time span in extraction kettle successively and are: 24min, 36min, 12min, 12min、12min、24min;Extracting pressure is 25MPa, and extraction temperature is 45 DEG C, and extraction time is 1.5h, and separating pressure is 6MPa, separation temperature is 45 DEG C, obtains seed of bark of eucommia crude oil.
(2) seed of bark of eucommia crude oil refine.
(2-1) being placed in heating tank by seed of bark of eucommia crude oil, be warming up to 60 DEG C, adding weight is seed of bark of eucommia crude oil weight 0.05wt ‰, concentration are the phosphoric acid of 80wt%, react 45min.
(2-2) the seed of bark of eucommia crude oil in heating tank is proceeded in outer tank, add the aqueous slkali prepared in advance immediately, predominate Entering alkali liquor at the uniform velocity to stir on one side, mixing speed is 40 turns/min, reacts 10min, settles 4h.
Alkali liquor is NaOH solution, and NaOH solution is 3:1mL/g with the ratio of seed of bark of eucommia crude oil;Alkalization temperature is 70 DEG C.Always Alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are Kg/h for oil flow, unit, and AV is seed of bark of eucommia crude oil Acid number, unit be mgNaOH/g.
B. phosphoric acid alkali consumption NP: owing to the addition of phosphoric acid in the degumming of this technique, therefore alkali liquor interpolation is considered as neutralising phosphoric acid consumption Alkali number;NP=1.22 × W, W are H3PO4Addition, unit are Kg/h, and the amount of phosphoric acid is pure phosphoric acid amount here.
C. excess alkali quantity NC: excess alkali is the 0.5wt% of oil mass, NC=Q × 50%, and Q is Kg/h for oil flow, unit.
Actual caustic soda amount NS: due to the Caustic soda purity on market, therefore should be according to its NaOH actual content when calculating Convert: the NaOH percentage composition of actual caustic soda amount NS=(N+NP+NC)/commercially available alkali.
(2-3) taking supernatant, adding NaCl mass fraction is the NaCl solution of 0.5wt%, and NaCl solution addition is Du Secondary seed crude oil weight 5wt%, at the uniform velocity stirs, 40 turns/min of rotating speed, settles 2h.
(2-4) take supernatant, vacuum be 0.06Mpa, temperature be 90 DEG C under conditions of be dried.
(2-5) enter bleacher, in bleacher vacuum be 0.06Mpa, temperature be 90 DEG C, toward bleacher in addition the Cortex Eucommiae The food grade active hargil of seed crude oil weight 2wt%, reacts 45min.
(2-6) open circulated filter system, be circulated filtration, clarifying to seed of bark of eucommia crude oil.
(2-7) enter in deodorizing tower, in deodorizing tower vacuum be 0.0002MPa, temperature be 120 DEG C, react 3h;Deodorizing tower It is to use physical refining tower and fatty acid supplementary set device to be applied in combination and carry out physical deacidification deodorize.
(2-8) being naturally cooling to 100 DEG C, water flowing is accelerated to be cooled to room temperature.
(2-9) carry out polishing by bag filter to filter, and gave the pressure of 4kg, filter, obtain seed of bark of eucommia essence Oil refining;In bag filter, the material of filter bag film is polyphenylene sulfide fibre;The aperture size of filter bag film in bag filter For 0.2nm.
Palmic acid, stearic acid, oleic acid, the content of linoleic acid plus linolenic acid and Folium Persicae coral in the seed of bark of eucommia refined oil obtained The coral glycosides proportion of goods damageds are as shown in table 1-1;The seed of bark of eucommia refined oil physicochemical property obtained is as shown in table 1-2.
The aucubin proportion of goods damageds=(aucubin in the quality seed of bark of eucommia refined oil of aucubin in seed of bark of eucommia Quality) quality * 100% of aucubin in/seed of bark of eucommia, aucubin content (mg/100g) and Du in seed of bark of eucommia In secondary seed refined oil, aucubin content (mg/100g) all uses detection method well known in the prior art.
The seed of bark of eucommia refined oil fatty acid that table 1-1 obtains forms and content
Note: the seed of bark of eucommia crude oil aerial shelf-life is less than three months.
The seed of bark of eucommia refined oil physicochemical property that table 1-2 obtains
* it is crude oil and the refined oil of corresponding embodiment extraction
The preparation of Part II mountain almond oil
A kind of mountain almond oil extracts refinery practice, comprises the steps:
(1) the de-bitter pre-treatment of Semen pruni armeniacae.
(1-1) Semen pruni armeniacae hulling machine shelling, first machine screening, then artificial screening obtains the Semen pruni armeniacae that shells;
(1-2) Semen pruni armeniacae is poured 120s in 100 DEG C of hot water into, proceed to 10 DEG C of cold water impinging cooling 5min;
(1-3) being poured into by Semen pruni armeniacae in stripping machine and peel, first machine screening, then artificial screening obtains Prunus armeniaca L.var.ansu Maxim. of peeling Core;
(1-4) decortication Semen pruni armeniacae is poured in 100 DEG C of hot water carry out four times soak, water temperature natural cooling in immersion process; Soak 4h for the first time, rinse with tap water after pulling out;Second time soaks 12h, rinses with tap water after pulling out;Third time is soaked 4h, rinses with tap water after pulling out;Soak 4h, rinse with tap water after pulling out for 4th time;
(1-5) pouring in drying pool by the Semen pruni armeniacae of de-hardship, at 70 DEG C, microwave drying, the frequency of microwave drying is 2400MHz, power 2500W, the thickness of the bed of material is 6cm.
(2) mountain almond oil extracts refine.
Mountain almond oil extracts refine and includes that low temperature pressing extracts mountain almond oil and mountain almond oil refine;
(2-1) pretreatment after Semen pruni armeniacae takes off hardship: before low temperature pressing extracts mountain almond oil, first Semen pruni armeniacae was pulverized 50 mesh sieves obtain Semen pruni armeniacae powder, Semen pruni armeniacae powder is immersed in temperature be 60 DEG C, polyvinyl alcohol mass fraction be 3wt%, Polyethylene Glycol Mass fraction be 10wt% polyvinyl alcohol-polyethylene glycol solution in 1 hour, Semen pruni armeniacae powder soak while carry out ultrasonic place Reason, ultrasonic power is 350W, supersonic frequency 40KHz, filters and is dried to obtain Semen pruni armeniacae powder, and polyvinyl alcohol is polyvinyl alcohol 1799, Polyethylene Glycol is PEG400;
The preparation method of polyvinyl alcohol-polyethylene glycol solution is as follows: polyvinyl alcohol 1799 is soaked in ethanol mass fraction For in the ethanol solution of 85wt% 12 hours, filtering drying, then the polyvinyl alcohol obtained is joined in the water of 60 DEG C, heating Stir 1 hour to obtain poly-vinyl alcohol solution, obtain polyvinyl alcohol-polyethylene glycol after then adding PEG400 stirring and dissolving molten Liquid;
(2-2) during low temperature pressing extracts mountain almond oil step: expressing process uses pure physical squeezing, and temperature controls 55 DEG C, solid-liquid is carried out the isolated Semen pruni armeniacae dregs of rice and supernatant.Then Semen pruni armeniacae dregs of rice post processing is carried out: joined by the Semen pruni armeniacae dregs of rice In the water of its quality 4 times, utilizing microwave reactor to control the temperature 60 C of material, the frequency of microwave reactor is 3000MHz, merit Rate 2500W, then to be added thereto to account for Semen pruni armeniacae dregs of rice mass fraction be the compound enzyme of 0.065wt%, enzymolysis 80min, slightly centrifugal Semen pruni armeniacae crude oil;Compound enzyme includes that the mass ratio of protease and cellulase, protease and cellulase is 1:3;Protease bag The mass ratio including neutral protease and alkaline protease, neutral protease and alkaline protease is 2:3.
(2-3) mountain almond oil refine:
(2-3-1) supernatant obtained in and the mixing of thick Semen pruni armeniacae crude oil, obtain Semen pruni armeniacae crude oil;
(2-3-2) Semen pruni armeniacae crude oil being warming up to 70 DEG C, addition Semen pruni armeniacae crude oil weight 0.15wt%, concentration are 80wt%'s Phosphoric acid, reacts 35min;
(2-3-3) take the supernatant obtained in step (2-3-2), add the water of Semen pruni armeniacae crude oil weight 15wt%, at the uniform velocity stir Mixing, rotating speed is 50 turns/min, settles 2h;
(2-3-4) take the supernatant obtained in step (2-3-3), vacuum be 0.095Mpa, temperature be the bar of 90 DEG C It is dried under part;
(2-3-5) enter bleacher, in bleacher vacuum be 0.095Mpa, temperature be 90 DEG C, add Semen pruni armeniacae crude oil The food grade active hargil of weight 4wt%, reacts 35min;
(2-3-6) open circulated filter system, be circulated filtration, clarifying to filter liquor;
(2-3-7) enter in deodorizing tower, in deodorizing tower vacuum be 0.0002MPa, temperature be 110 DEG C, react 2h;
(2-3-8) being naturally cooling to 100 DEG C, water flowing is accelerated to be cooled to room temperature;
(2-3-9) it is polished filtering by bag filter, gives the pressure of 4kg, filter, obtain Semen pruni armeniacae Refined oil.
Gained Semen pruni armeniacae refined oil fatty acid composition, content analysis and physicochemical property are as shown in table 2-1 and table 2-2.
Table 2-1 Semen pruni armeniacae refined oil fatty acid composition and content analysis
Table 2-2 Semen pruni armeniacae refined oil physicochemical property
The preparation of Part III Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil
Mountain almond oil and eucommia ulmoides seed oil used by this part use the eucommia ulmoides seed oil and second prepared by above-mentioned Part I The mountain almond oil of part preparation.
Embodiment 1
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, including the component of following mass fraction:
The mixture (volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 3:1) 2.0% of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil, vitamin E acetate 0.5%, GTCC30%, ethylhexyl palmitate 40%, olive oil 27.2%, essence 0.02% and PE9010 0.28%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 80 DEG C, and pressure is 18 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Embodiment 2
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, including the component of following mass fraction:
The mixture (volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 4:1) 1.5% of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil, vitamin E acetate 0.435%, GTCC30.7%, ethylhexyl palmitate 40%, olive oil 27%, essence 0.025% and PE9010 0.34%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 75 DEG C, pressure 20 handkerchief;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Embodiment 3
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, including the component of following mass fraction:
The mixture (volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 5:1) 2.8% of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil, vitamin E acetate 0.6%, GTCC26.3%, ethylhexyl palmitate 38%, olive oil 32%, essence 0.030% and PE9010 0.27%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 85 DEG C, pressure 15 handkerchief;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Embodiment 4
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, including the component of following mass fraction:
The mixture (volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 1:1) 2.952% of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil, vitamin E acetate 0.3%, GTCC30%, ethylhexyl palmitate 44.5%, olive oil 22%, essence 0.016% and PE9010 0.232%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 70 DEG C, and pressure is 13 handkerchiefs;
(2) raw materials such as emollient and preservative Prunus armeniaca L.var.ansu Maxim. oil/eucommia ulmoides seed oil are joined in vacuum emulsification pot, stirring?Time, Raw material mix homogeneously is made i.e. to obtain product.
Comparative example 1
Prunus armeniaca L.var.ansu Maxim. massage oil, including the component of following mass fraction:
Prunus armeniaca L.var.ansu Maxim. oil 1.98%, vitamin E acetate 0.5%, GTCC30%, ethylhexyl palmitate 40%, olive oil 27.2%, Essence 0.02% and PE9010 0.3%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 80 DEG C, and pressure is 18 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Comparative example 2
Prunus armeniaca L.var.ansu Maxim. massage oil, including the component of following mass fraction:
Prunus armeniaca L.var.ansu Maxim. oil 3.0%, vitamin E acetate 0.48%, GTCC30%, ethylhexyl palmitate 40%, olive oil 26.2%, Essence 0.02% and PE9010 0.3%.
The preparation method of Prunus armeniaca L.var.ansu Maxim. massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 75 DEG C, pressure 20 handkerchief;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Comparative example 3
Cortex Eucommiae massage oil, including the component of following mass fraction:
Eucommia ulmoides seed oil 2.0%, vitamin E acetate 0.5%, GTCC29.98%, ethylhexyl palmitate 40%, olive oil 27.2%, essence 0.02% and PE9010 0.3%.
The preparation method of Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 85 DEG C, and pressure is 15 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Comparative example 4
Cortex Eucommiae massage oil, including the component of following mass fraction:
Eucommia ulmoides seed oil 3.0%, vitamin E acetate 0.5%, GTCC30%, ethylhexyl palmitate 40%, olive oil 26.18%, essence 0.02% and PE9010 0.3%.
The preparation method of Cortex Eucommiae massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 70 DEG C, and pressure is 13 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Comparative example 5
Massage oil, including the component of following mass fraction:
Vitamin E acetate 0.5%, GTCC30%, ethylhexyl palmitate 40%, olive oil 29.18%, essence 0.02% and PE9010 0.3%.
The preparation method of massage oil, comprises the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 80 DEG C, and pressure is 18 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
Embodiment 1-4 and comparative example 1-5 are on skin elasticity impact experiment:
Subject Population being divided into 9 groups, often organizes 20 people, each group of people uses embodiment 1~4 and the massage of comparative example 1~5 respectively Oil.
Before smearing massage oil, experimenter uses identical soap or handwashing liquid cleaning hand, experimenter right-hand man 3 × 3cm is selected in lateral symmetry position2Size area as test position, then left hand smear about 1g embodiment 1-4 by Rub oil, smears the product of equivalent comparative example 1-5 as comparison at the right hand, use frequency be early, middle and late each the most once, continuous every day Use, use 5 weeks continuously.
Use embodiment 1~4 and comparative example 1~5 massage oil before, at every experimenter's test zone skin bullet Property tester (Germany CK company produce, model MPA580) detection test position elasticity number N0Value, is repeated 5 times respectively, draws Meansigma methods.
Detecting the most respectively at these positions after using 1,2,3,4,5 weeks, each test zone respectively detects 10 hypoelasticity N Value, the skin elasticity test value as this time of averaging.Then test value is deducted the N not using sample0Value, then divided by N0It is worth to the Flexible change rate at this position, when Flexible change rate is the biggest, illustrates that sample is more conducive to the raising of skin elasticity. Embodiment 1~4 and the skin elasticity rate of change of comparative example 1~5 as shown in table 3-1:
Table 3-1
Embodiment 1 week (%) 2 weeks (%) 3 weeks (%) 4 weeks (%) 5 weeks (%)
Embodiment 1 18.3 36.9 41.8 50.2 68.5
Embodiment 2 10.6 29.4 35.6 45.8 55.4
Embodiment 3 11.7 30.5 36.2 44.1 52.6
Embodiment 4 13.5 33.8 39.7 46.8 62.4
Comparative example 1 6.5 19.8 27.6 38.7 43.6
Comparative example 2 7.4 20.5 29.4 40.1 45.3
Comparative example 3 7.9 17.9 32.4 41.5 48.3
Comparative example 4 8.4 22.6 35.6 43.8 50.7
To Billy 5 5.6 15.7 24.9 36.4 40.6
It follows that determine embodiment 1~4 and comparative example 1~5 massage oil oxidation stability, test result such as table 3-2 Shown in:
Table 3-2
From the results shown in Table 2, the massage oil oxidation stability of embodiment 1 is best, compared with comparative example 2 and 4, When the content of the massage oil of the proportioning that almond oil mixes with Eucommia Oil, especially almond oil and Eucommia Oil is 2%, it is oxidation-stabilized Property optimum.
Embodiment 1-4 and the toxicology test of comparative example 1-5:
The massage oil of embodiment 1-4 and comparative example 1-5 is carried out toxicology test detection.Testing conditions and result are as follows:
1. testing agency's title: certain inspection and quarantine bureau's inspection and quarantine complex art center;
2. inspected time: 2016.04.19;
3. detection foundation: " cosmetics health specification " (version in 2007);
4. testing result: repeatedly skin test irritation test result is: nonirritant.
Embodiment 1-4 and the repeatedly irritation test of comparative example 1-5:
The massage oil of embodiment 1-4 and comparative example 1-5 is carried out repeatedly irritation test.Testing conditions and result are such as Under:
1. testing agency's title: certain inspection and quarantine bureau's inspection and quarantine complex art center;
2. inspected time: 2016.04.19;
3. detection foundation: " cosmetics health specification " (version in 2007);
4. detection method and result:
4.1 tested material
4.2 animals and feeding environment
4.3 test method
Repeatedly irritation test is carried out according to " cosmetics health specification " (version in 2007);
Being cut by hair spinal column both sides, laboratory animal back before Shi Yan, unhairing scope is respectively 3cm × 3cm, surface covered 2.5cm×2.5cm。
Taking tested material 0.5mL to be coated on the skin of side, opposite side painting normal saline, as comparison, applies 1 time, even every day Continuous coating 14d.From the beginning of second day, it is coated with cropping before application every time, removes residual tested material with normal saline.
4.4 result of the test
Matched group does not occur in 1-14 days that erythema and edema, embodiment 1-4 and comparative example 1-5 did not had in 1-14 days yet Erythema and edema occur, by the skin irritation of rabbit is tested, have no other toxicity, further illustrate the application Fructus Pruni Core Cortex Eucommiae massage oil is nonirritant to rabbit repeatedly irritation test result.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not right The restriction of embodiments of the present invention, for those of ordinary skill in the field, the most also may be used To make other changes in different forms, cannot all of embodiment be given exhaustive here, every belong to this What bright technical scheme was extended out obviously changes or changes the row still in protection scope of the present invention.

Claims (10)

1. a Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, it is characterised in that be made up of following component: emollient and preservative.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 1, it is characterised in that described emollient includes Prunus armeniaca L.var.ansu Maxim. oil and the Cortex Eucommiae Mixture, vitamin E acetate, caprylic/capric triglyceride, ethylhexyl palmitate, olive oil and the essence of oil.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 1, it is characterised in that described preservative is phenyl phenol & second Base hexyl glycerol.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 1, it is characterised in that described emollient includes Prunus armeniaca L.var.ansu Maxim. oil and the Cortex Eucommiae Mixture, vitamin E acetate, caprylic/capric triglyceride, ethylhexyl palmitate, olive oil and the essence of oil;Described preservative For phenyl phenol & ethylhexyl glycerol.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 4, it is characterised in that be made up of the component of following mass fraction: Prunus armeniaca L.var.ansu Maxim. oil and the mixture 1.5 of Eucommia Oil~3.0%, vitamin E acetate 0.3~0.7%, caprylic/capric triglyceride 20~ 40%, ethylhexyl palmitate 30~50%, olive oil 20~35%, essence 0.014~0.035% and phenyl phenol & Ethylhexyl glycerol 0.21~0.38%.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 5, it is characterised in that the volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 6 ~0.2:1.
Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 6, it is characterised in that include the component of following mass fraction: mountain Fructus Pruni oil and the mixture 2.0% of Eucommia Oil, vitamin E acetate 0.5%, caprylic/capric triglyceride 30%, ethylhexyl palmitate 40%, olive oil 27.2%, essence 0.02% and phenyl phenol & ethylhexyl glycerol 0.28%, Prunus armeniaca L.var.ansu Maxim. oil and the Cortex Eucommiae In the mixture of oil, Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil volume ratio are 3:1.
8. the preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil, it is characterised in that comprise the steps:
(1) being dried by vacuum emulsification pot, the temperature of regulation vacuum emulsification pot is 80~85 DEG C, and pressure is 5~20 handkerchiefs;
(2) emollient and preservative are joined in vacuum emulsification pot, stirring, make raw material mix homogeneously i.e. obtain product.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 8, it is characterised in that described emollient includes mountain Fructus Pruni oil and the mixture of Eucommia Oil, vitamin E acetate, caprylic/capric triglyceride, ethylhexyl palmitate, olive oil and essence; Described preservative is phenyl phenol & ethylhexyl glycerol.
The preparation method of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil the most according to claim 9, it is characterised in that Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil Mixture 1.5~3.0%, vitamin E acetate 0.3~0.7%, caprylic/capric triglyceride 20~40%, palm acid ethyl oneself Ester 30~50%, olive oil 20~35%, essence 0.014~0.035% and phenyl phenol & ethylhexyl glycerol 0.21~0.38%;The volume ratio of Prunus armeniaca L.var.ansu Maxim. oil and Eucommia Oil is 6~0.2:1.
CN201610515437.8A 2016-07-02 2016-07-02 A kind of Prunus armeniaca L.var.ansu Maxim. Cortex Eucommiae massage oil and preparation method thereof Pending CN106256340A (en)

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